CHINESE JOURNAL OF ENERGETIC MATERIALS
+高级检索
基于连续流微反应器的3,4-二硝基-1H-吡唑的VNS胺化反应工艺优化与动力学研究
作者:
作者单位:

南京理工大学化学与化工学院, 江苏 南京 210094

作者简介:

通讯作者:

基金项目:

国家自然科学基金(22305121)


Process Optimization and Kinetic Study of VNS Amination of 3,4-Dinitro-1H-pyrazole in a Continuous Flow Microreactor
Author:
Affiliation:

School of Chemistry and Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 支撑附件
    摘要:

    针对3,4-二硝基-1H-吡唑的替代亲核取代(VNS)胺化反应在传统间歇工艺中存在的反应低效、安全性差等问题,通过连续流微反应器技术,开展其VNS胺化合成工艺与反应动力学研究,系统考察了温度、流速及停留时间等关键参数对VNS胺化反应的影响。结果表明,反应的最优工艺为物料摩尔比4-氨基-4H-1,2,4-三唑:3,4-二硝基-1H-吡唑=3.6∶1、温度60 ℃、流速50 mL·min-1、停留时间105 s,该条件下VNS胺化反应产率最高达71%,且反应时间由30 min显著缩短至105 s。动力学研究表明,该VNS胺化反应符合一级动力学模型,活化能为15.50 kJ·mol-1,所拟合动力学模型与实验结果验证,在30~60 ℃温度范围内吻合良好。

    Abstract:

    To address the issues of low reaction efficiency and poor safety in the traditional batch process for the alternative nucleophilic substitution (VNS) amination of 3,4-dinitro-1H-pyrazole, this study employed continuous flow microreactor technology to investigate its VNS amination synthesis process and reaction kinetics. Key parameters such as temperature, feed flow rate, and residence time were systematically examined for their effects on the VNS amination reaction. The optimal reaction conditions were determined as a molar ratio of 4-amino-4H-1,2,4-triazole∶3,4-dinitro-1H-pyrazole = 3.6∶1, temperature of 60 ℃, flow rate of 50 mL·min-1, and residence time of 105 s, achieving a maximum yield of 71% with reaction time significantly reduced from 30 min to 105 s. Kinetic studies showed that the VNS amination reaction followed a first-order kinetic model, with an activation energy of 15.50 kJ·mol-1; the fitted kinetic model was well-constrained by experimental data across the temperature range of 30-60 ℃.

    参考文献
    相似文献
    引证文献
文章指标
  • PDF下载次数:
  • HTML阅读次数:
  • 摘要点击次数:
  • 引用次数:
引用本文

谭旭辰,曾志伟,唐明杰,等. 基于连续流微反应器的3,4-二硝基-1H-吡唑的VNS胺化反应工艺优化与动力学研究[J]. 含能材料,DOI:10.11943/CJEM2026081.

复制
历史
  • 收稿日期: 2026-04-03
  • 最后修改日期: 2026-07-16
  • 录用日期: 2026-07-09
  • 在线发布日期: 2026-07-14
  • 出版日期: